Volatile magnesium compounds and process of producing same.



UNITED STATES @FFEOE SAMUEL PEACOCK, 0F PHILADELPHIA, PENNSYLVANIA, ASSIGNOR, BY MESNE ASSIGN- MENTS, TO AGRICULTURAL RESEARCH CORPORATION, OF NEW YORK, N. Y., A

CORPORATION OF NEW YORK.

VOLATILE MAGNESI IUM COMPOUNDS AND PROCESS OF PRODUCING SAME.

il,ll3 l,4l12,

No Drawing.

To all whom it may concern Be it known that I, SAMUEL IEAoocK, a

citizen of the United States, residing at Philadelphia; in the county of Philadelphia and State of Pennsylvania, have invented certain new and useful Improvements 1n Volatile Magnesium Compounds 'and Processes of Producing Same; and I do hereby declare the following to be a full, clear, and exact description of the invention, such as will enable others skilled in the art to which it appertains to make and use the same. I

This invention relates to aprocess of {iroducing a volatile compound of carbon, nitrogen and magnesium from an oXid of magnesium, gaseous nitrogen and carbon.

My invention also relates to the new volatile product produced by this process and has for its object the fixation of free nitrogen in a manner more etlicient and less expensive than the methods heretofore proposed.

l/Vith these and other objects in view the invention consists in the new product and novel steps constituting my process more fully hereinafter disclosed and particularly pointed out in the claims.

In carrying out my process I. prepare a charge of finely divided oxid of magnesium and carbon, suitably proportion the same, and preferably briquet the said charge. I then introduce the charge into a suitable furnace. Gaseous nitrogen, or producer gas is introduced into the furnace chamber; and an electric current is turnedon, or other suitable heating means is employed, to raise the temperature to say substantially 1500 0., whereupon I have reason to believe the following reaction takes place I have now discovered that the carbonitrid thus formed in the high temperature zone of the furnace is in a volatile as well as in a solid form, and that the proportion of volatile to solid product depends in a measure upon the pressure existing in the furnace at the time-of formation. In other words, I have discovered that when the furnace pressure is above that of the atmosphere the proportion of volatile to solid carbo-nitrid produced is less than is the case when the pressure is that of the atmosphere; and that when the pressure is less than that of the .Specification of Letters Patent.

Patented Apr, 6, 19115.

Application filed April 18. 1914. Serial No. 832,810.

atmosphere the proportion of volatile product is greater than is the case when the atmospheric pressures exists in the furnace. For example when the pressure in the furnace is maintained for 80 minutes at 1000 m. in. of mercury, about 75% of the carbonitrid formed is volatilized while the remainder was found as a solid in the charge; when the pressure is maintained at 760 m. m.

for the same period substantially all the carbo-nitrid is volatilized; and when the pressure is less than thatof the atmosphere all the carbonitrid is volatilized in a period of time less than 30 minutes.

Either nitrogen gas or producer gas may be employed as above'stated, and when producer gas is employed such gas may contain on the average about 60% nitrogen, N,, and 38% carbon monoxid, CO, so that when the nitrogen is removed by my process the producer gas is greatly improved and enriched by the carbon monoXid CO. enerated by the reaction. Therefore, said producer gas after coming from the furnace can later be utilized to a greater advantage for combustion or other purposes. That is to say, from the carbo-nitrid equation, above, it is evident that for each volume of nitrogen fixed, an equal volume of carbon monoxid CO. is liberated, and joins the furnace gases. Now when producer gas is employed, having say 60% of nitrogen and 38% of carbon monoxid, and when one third or 20% of the nitrogen is fixed, it is evident that 20% of carbon monoxid will still be added to the 38% of carbon monoxid already present. Accordingly the resulting mixture will contain 58% of carbon monoxid instead of its original 38%. It follows, therefore, that the producer gas by my process is not only purified of its nitrogen but it is also enriched. by a substantial addition of carbon monoXid, causing it to become a valuable by-product. In carrying out the process in order to avoid a serious retardation of the reaction it is desirable to maintain such a flow of nitrogen through the furnace that the partial pressure of the carbon monoxid gas present will not exceed say 350 to 400 millimeters of mercury. The volatile carbo-nitrid thus produced may be recovered by leadin it from the furnace and allowing it to soli ify or condense in suitable chambers, or by absorption in water or other solutions, if re covered by condensation, the solid-thus ob water in a suitably closed vessel at substantiblly 200 (3., when the following reaction tion, the combined nitrogen inay be convert ed into ammonia, by heating the solu-tion'to substantially 200 C. in a suitably closed .vessel. If the volatile product 'is allowed to condense as a loose powder when recovering it,- it is apt to absorb any moisture with which it mi ht come in contact. and also to rapidly oxldize if exposed to free oxygen, and therefore care should be taken to prevent the exposure of this new product to water vapor or to the atmosphere.

In actual tests usingmagnesium oxid, carbon and nitrogen gas and atemperature of 1500 C. for 3.0 minutes analyses show that I over 80% of the magnesium. present in the magnesium oxid carried by the charge appeared in the volatile carbo nitrid' produced. These analyses further show chemically-combined nitrogen as wellas chemically com 'bined carbon in the volatilized products in the Mg N C N f It is therefore "certain that my volatile product is a carbo-nitrid and not a nitrid. The solid portion of the carbo-nitrid which .is formed simultaneously-with the volatile portion remains in the residue passing through the furnace and its combined' nitrogen may be; recovered in the form. of ammonia by treating said. residue with water at about/200 C; in a suitably closed vessels v The reactions of my new volatile product when hydrolyzed leads to the supposition. "that it produces a polymer of cyanamid in that it gives some of the characteristic reaction of melamin, such as a white precipitate with soluble silver and lead salts.

It is obvious that those skilled in the art may vary the details of my rocess without departing from the spirit o my invention, andtherefore I do not wish to be limited to the abovedisclosure except as may be requiredby the claims.

What I claim is},- 1.

1. The process of producing a. volatile "magnesium carbo-nitrid, which consists in preparing a mixture of ma esium oxid and carbon; and subjecting said mixture in an atmospherecontainingfree nitrogen to a void of chemically proportion required by the formula temperature sufiicient to produce said vola tained may be subjected to the action oftile .carbo-nitrid, substantially as described.

2. The process of producing a volatile magnesium carbo-nitrid which-consists in preparing amixture of magnesium oxid and carbon; subjecting said mixture in an ata s mosphere containing nitrogen to a ter'npera- If the carbo-n1tr1d is recovered as a solu-' ture sufiic'ient to produce said carbo-nitri'd',

and recovering thelatter in a-medium deactive oxygen, s'ubstanv tially -'as described.

3. The process of producing a volatile magnesium carbo-nitrid which consists in "preparinga mixture of magnesium oxid and .carbon; subjecting said mixture in anatmos: phere of producer gas to atemperature' s'uf- -ficient to produce said carbo-nitrid, and re-- covering the latter in a mediumdevoid of. v chemically. active oxygen, substantially as.

described.

4. The process ofproducing a volatile magnesium carbo-nitrld, which consists 80.

preparing a-mixture of magnesium oxid and carbon; and subjecting the same in an atmosphere containing nitrogen to'a temperature sufiicient to produce said carbo-nitridthereby causing carbon-monoxid to. be

evolved while maintaining the partial pres-,isfi

"sure of the carbon; monoxid present below 400 millimeters of mercury, substantiallyas described.

, 5, The herein described new product con 1 a taining chemicallycombined carbon nitro-' "gen and magnesium the-same being volatile,

at1500 .C., capable ofgfor'ming a soluble white powder and vof producing a white-"- precipitate with soluble silver and lead salts,

as well as producing'ammonia when sub- .jected to the action of hotiwater, substan-' tiallyasde'sc'ribed.

6., The process of fixing nitrogen and si multaneously enriching producer gas which consists in providin at mixture of magnesium oxid and car on; feeding producer gas. containing nitrogen thereto; and raising the temperature of said mixture su'fiiciently to cause some of said nitrogen .to"beremoved from'said gas by combining with ma sium and carbon whilealso causing the carbon monoxid evolved to be added to the. said producer gas, substantially as described.

In testimony whereof I afiix-my signature, in'presence of two witnesses. I

f SAMUEL PEACOCK';

Witnesses:

.T, A. Wrrminsr'oox,

FRANoEs. Smear;

qopl el' e f this patent may be obtaine'd tor five cents each, by addressing thc- (commissioner of Intent,

I wnhingtomfl. 

